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Tuning and validation of an extraction and chromatography method for omeprazole in drug formulations

Coto Acosta, Mar LU (2016) KEMR16 20152
Department of Chemistry
Abstract
Gastric ulcer is a common disorder in horses. A known potent inhibitor of gastric acid secretion is omeprazole. This thesis describes the study of omeprazole extraction followed by a high-performance liquid chromatography (HPLC) method for the quantification of omeprazole in enteric-coated pellets (raw material) and in oral paste (final drug product) for horses. The drug product is composed by a paste in which pellets are wrapped. The reason for this investigation is the absence of a proper methodology applicable to the pharmaceutical industry and the necessity to determine the trueness of the method. In the first place, HPLC was validated using a reference standard of omeprazole. The method showed results within acceptable criteria in... (More)
Gastric ulcer is a common disorder in horses. A known potent inhibitor of gastric acid secretion is omeprazole. This thesis describes the study of omeprazole extraction followed by a high-performance liquid chromatography (HPLC) method for the quantification of omeprazole in enteric-coated pellets (raw material) and in oral paste (final drug product) for horses. The drug product is composed by a paste in which pellets are wrapped. The reason for this investigation is the absence of a proper methodology applicable to the pharmaceutical industry and the necessity to determine the trueness of the method. In the first place, HPLC was validated using a reference standard of omeprazole. The method showed results within acceptable criteria in comparison with the intervals established by the United States Pharmacopeia (USP) for analytical parameters such as linearity (r2=0.9998) and precision (RSD 0.38%). Secondly, the experimental design for the extraction method of omeprazole from pellets was performed by trying a range of extraction conditions, such as the use of magnetic stirring and different sonication times. Extraction of omeprazole method from oral paste was already developed but it needed to be studied deeper. However, when the chromatographic method was applied to raw materials and drug product, higher concentration values than expected were obtained (e.g. 230.66 μg/ml omeprazole in pellets instead of the 220 μg/ml expected). A reason for such high values could be related to systematic errors and the instability of the pellets. Dimensions of pellets, the coating thickness and/or the size of inert core of the pellets can vary and thereby be sources of possible variation. Trueness of the method remains unknown because there is a lack of knowledge about the real concentration value and further studies are needed. (Less)
Popular Abstract
A new formulation to be administered in horses has been recently developed. This drug is called omeprazole and it was discovered to be successful for the treatment of gastric ulcers in horses, a common illness in race-horses. A high performance liquid chromatography (HPLC) quantification method was studied with the aim to validate a method for the determination of omeprazole in pharmaceutical samples. Due to the absence of an efficient extraction method of omeprazole, a sample preparation method was also studied.
Chromatography is a well-known separation technique which is widely used in analytical laboratories. Analytical chromatography is done to separate particular substances. One type of chromatography technique is HPLC. In general... (More)
A new formulation to be administered in horses has been recently developed. This drug is called omeprazole and it was discovered to be successful for the treatment of gastric ulcers in horses, a common illness in race-horses. A high performance liquid chromatography (HPLC) quantification method was studied with the aim to validate a method for the determination of omeprazole in pharmaceutical samples. Due to the absence of an efficient extraction method of omeprazole, a sample preparation method was also studied.
Chromatography is a well-known separation technique which is widely used in analytical laboratories. Analytical chromatography is done to separate particular substances. One type of chromatography technique is HPLC. In general terms, a mixture composed by different substances is injected into a liquid (mobile phase) that flows through the chromatography system (stationary phase); separation is achieved due to chemical and physical interactions between both phases. Depending on the compounds adsorption with the stationary phase, they will spend different times in the column; so compounds will elute according to their affinity.
In this study, once the chromatographic method was evaluated for different analytical parameters, it was applied to drug formulations. From previous research, it is known the need of an efficient sample preparation. So, different lab techniques were tried to ensure the total extraction of omeprazole from the formulations previous to its HPLC quantification.
Finally, some inconsistencies were found because higher values than established in the label claim were obtained. A possible reason for such differences could be related with physical instability of the samples and errors introduced during the different steps of the experiments. (Less)
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author
Coto Acosta, Mar LU
supervisor
organization
course
KEMR16 20152
year
type
H2 - Master's Degree (Two Years)
subject
keywords
Extraction methods, Omeprazole, Horses, Analytical Chemistry, Anti-ulcer drugs, HPLC, Validation, analytisk kemi
language
English
id
8871997
date added to LUP
2016-05-27 15:46:53
date last changed
2016-05-27 15:46:53
@misc{8871997,
  abstract     = {Gastric ulcer is a common disorder in horses. A known potent inhibitor of gastric acid secretion is omeprazole. This thesis describes the study of omeprazole extraction followed by a high-performance liquid chromatography (HPLC) method for the quantification of omeprazole in enteric-coated pellets (raw material) and in oral paste (final drug product) for horses. The drug product is composed by a paste in which pellets are wrapped. The reason for this investigation is the absence of a proper methodology applicable to the pharmaceutical industry and the necessity to determine the trueness of the method. In the first place, HPLC was validated using a reference standard of omeprazole. The method showed results within acceptable criteria in comparison with the intervals established by the United States Pharmacopeia (USP) for analytical parameters such as linearity (r2=0.9998) and precision (RSD 0.38%). Secondly, the experimental design for the extraction method of omeprazole from pellets was performed by trying a range of extraction conditions, such as the use of magnetic stirring and different sonication times. Extraction of omeprazole method from oral paste was already developed but it needed to be studied deeper. However, when the chromatographic method was applied to raw materials and drug product, higher concentration values than expected were obtained (e.g. 230.66 μg/ml omeprazole in pellets instead of the 220 μg/ml expected). A reason for such high values could be related to systematic errors and the instability of the pellets. Dimensions of pellets, the coating thickness and/or the size of inert core of the pellets can vary and thereby be sources of possible variation. Trueness of the method remains unknown because there is a lack of knowledge about the real concentration value and further studies are needed.},
  author       = {Coto Acosta, Mar},
  keyword      = {Extraction methods,Omeprazole,Horses,Analytical Chemistry,Anti-ulcer drugs,HPLC,Validation,analytisk kemi},
  language     = {eng},
  note         = {Student Paper},
  title        = {Tuning and validation of an extraction and chromatography method for omeprazole in drug formulations},
  year         = {2016},
}